CN106589207A - Electrolyte-resistant pigment printing thickener - Google Patents
Electrolyte-resistant pigment printing thickener Download PDFInfo
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- CN106589207A CN106589207A CN201611107218.2A CN201611107218A CN106589207A CN 106589207 A CN106589207 A CN 106589207A CN 201611107218 A CN201611107218 A CN 201611107218A CN 106589207 A CN106589207 A CN 106589207A
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- Prior art keywords
- electrolyte
- agent
- thickener
- resistant
- initiator
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/52—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing synthetic macromolecular substances
- D06P1/5207—Macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- D06P1/525—Polymers of unsaturated carboxylic acids or functional derivatives thereof
- D06P1/5257—(Meth)acrylic acid
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses an electrolyte-resistant pigment printing thickener, belongs to the technical field of textile dyeing and printing auxiliaries, and aims to solve the problem of poor electrolyte resistance and thickening effect coordination of the conventional printing acrylic acid synthetic thickener. The electrolyte-resistant pigment printing thickener is obtained by neutralizing an acrylic acid monomer with a pH conditioner, adding an initiator ammonium persulfate and a crosslinking agent to prepare an aqueous phase, carrying out pre-emulsification the aqueous phase and an oil phase prepared from an oil-phase solvent, an initiator, an emulsifier and a comonomer, further performing complete emulsification under the action of an initiator sodium bisulfite, finally adding a reversed-phase emulsifier for complete reversed-phase emulsification and performing discharging and drying. The prepared electrolyte-resistant pigment printing thickener has high thickening performance and electrolyte resistance, and is simple in preparation process and easy to be industrially produced.
Description
Technical field
The present invention relates to a kind of thickening agent, more particularly to a kind of paint thickener for printing of electrolyte-resistant.
Background technology
Pigment printing is that finely divided granules of pigments is bonded at printing method on fabric by the effect of binding agent, is had
Processing technique is simple, without steaming, " three wastes " are few the features such as.In pigment printing, by thickening agent, water, binding agent and coating group
Into paint-printing colour size, in the presence of printing machine scraper, shearing force is produced to it, make the viscosity of print paste big in moment
Amplitude reduction, is printed on fabric after half tone, when shearing force disappears, original high viscosity is returned to again, prints fabric
Spend clear-cut, this viscosity occurred with the size variation of shearing force changes, and mainly realizes by thickening agent.
Patent CN103450423B introduces maleic anhydride modified shitosan to improve thickening agent using reversed-phase emulsion copolymerization method
Electrolyte resistance, by the method increasing thickening agent electrolyte resistance, and easily industrialization, but its thickening effect agent plus
8000-9000mpas is can only achieve after entering relatively low, thickening effect is not so good.
Patent CN101886345A prepares anionic acrylic monomer class thickening agent using reversed-phase emulsion copolymerization method, at it
Molecule segment introduces polyether segment and using micro- crosslinking technological so as to which electrolyte-resistant and an armful aqueouss have been improved, but it is prepared
The monomer component of raw material is complicated, and condition is wayward, and thickening effect is not still good enough.
Patent CN101538807A is prepared for a kind of anionic acrylic monomer class thickening using reversed emulsion polymerization
Agent, by introducing tertiary amine group and vinyl group in the segment of polymer, improves the electrolyte-resistant ability of thickening agent and embraces
Outlet capacity, but thickening effect is not good enough.
Patent CN1056659C discloses one kind
The method that main body inverse emulsion polymerization prepares the printing thickening agent for being mainly used in textile product stamp field.Press in aggregation container
Ratio adds raw material, and nitrogen is passed through under stirring condition side by side except oxygen, is polymerized under conditions of 20-80 DEG C of constant temperature, the increasing of product
Thick ability is general, and its electrolyte-resistant ability and tinctorial yield equally comply with one's wishes not to the utmost.
Patent CN101619543B discloses one kind by acrylic acid, acrylamide, 25% ammonia, function monomer, initiator
Textile printing thickening agent has been synthesized using inverse emulsion polymerization Deng raw material.The thickening agent has good thickening effect, but its resistance to electricity
Solution matter performance is still improved seldom.
The content of the invention
It is an object of the invention to overcome existing stamp acrylic acid seriess synthetic thickening agent electrolyte-resistant ability and thickening
The problem of effect inaccurate coordination, there is provided a kind of thickening effect is good and acrylic acid reversed-phase emulsion with good electrolyte-resistant ability gathers
The printing thickening agent of conjunction.
The technical scheme is that：A kind of paint thickener for printing of electrolyte-resistant, the thickening agent by acrylic monomerss,
PH adjusting agent, oil phase solvent, cross-linking agent, initiator, emulsifying agent, rp-emulsification agent, comonomer synthesis, by weight, its
Consist of：
The PH regulators are 20-30% sodium hydroxide solutions.
The oil phase solvent is tasteless kerosene.
The cross-linking agent is N, the double ammonium of N- methylene acrylic acid.
The initiator is Ammonium persulfate. and sodium sulfite.
The emulsifying agent is span-80.
The rp-emulsification agent is Tween-80.
The comonomer is the fat of acrylic acid 18.
By such scheme, the preparation method of the paint thickener for printing of described electrolyte-resistant is comprised the following steps：
(1) under conditions of stirring, PH regulators are slowly added dropwise, acrylic monomerss is neutralized, persistently stirring makes neutralization temperature
Degree is less than 40 DEG C.
(2) initiator ammonium persulfate and cross-linking agent are added in the solution neutralized to step (1), water phase is obtained.
(3) oil phase solvent, emulsifying agent and comonomer are mixed, high-speed stirred obtains oil phase.
(4) the oil phase mixing that the water phase and step (3) for obtaining step (2) is obtained, high speed emulsifying obtains pre-emulsion.
(5) under nitrogen protection, pour the pre-emulsion that step (4) is obtained into four-hole boiling flask stirring, be slowly added to cause
Agent sodium sulfite, is warming up to 65 DEG C of reaction 3h, then cools to 45 DEG C, adds rp-emulsification agent, reacts half an hour, then discharges
It is drying to obtain the acrylic thickener of electrolyte-resistant.
By such scheme, use by the electrolyte-resistant thickener is diluted with water to into 1%-5%.
The invention has the advantages that：
1st, a kind of electrolyte-resistant paint thickener for printing prepared by the present invention is faint yellow solid, can be with the water of various ratios
Mixing, under less volume, white slurry viscosity is up to 30000mpas, and thickening properties are good, and relative to commercially available PTF thickening agents, its
Electrolyte-resistant ability is significantly improved, and advantageously reduces use cost.
2nd, the present invention is as comonomer and its is molten in oil phase using octadecyl acrylate, on the one hand, can avoid gathering
There is sudden and violent poly- phenomenon in conjunction process, and on the other hand, it can be carried out well under initiator and uniform temperature with the acrylic acid in water phase
Random copolymerization, introduce hydrophobicity long-chained monomer, effectively improve the electrolyte-resistant ability of made thickening agent.
3rd, the present invention adopts Ammonium persulfate. and sodium sulfite as initiator, and substep adds, and can make thickening agent each group
Segregation is closed and carried out at a lower temperature so that stable reaction is gentle, is conducive to increasing the molecular weight of made thickening agent, improves it
Thickening effect.
4th, the present invention prepares thickening agent using inverse emulsion polymerization method, is conducive to improving polymerization stability and product storage
Stability, and present invention polymerization oil phase and watr-proportion are moderate, can further improve product stability.
5th, preparation process is simple of the present invention, production process is easily controlled, and is conducive to industrialized production.
Specific embodiment
In order to be better understood from the present invention, the present invention is further described below by embodiment, embodiment is only used
In the present invention is explained, any restriction is not constituted to the present invention.
Embodiment 1
A kind of paint thickener for printing of electrolyte-resistant, by weight, including following components：
20 parts of acrylic monomerss；
35.5 parts of PH regulators；
16 parts of oil phase solvent；
0.03 part of cross-linking agent；
0.08 part of initiator；
1.6 parts of emulsifying agent；
1.6 parts of rp-emulsification agent；
0.42 part of comonomer；
Its preparation method is comprised the following steps：
(1) under conditions of stirring, PH regulators are slowly added dropwise, acrylic monomerss is neutralized to, persistently stirring makes neutralization
Temperature is less than 40 DEG C.
(2) initiator ammonium persulfate and cross-linking agent are added in the solution neutralized to step (1), water phase is obtained.
(3) oil phase solvent, emulsifying agent and comonomer are mixed, high-speed stirred obtains oil phase.
(4) the oil phase mixing that the water phase and step (3) for obtaining step (2) is obtained, high speed emulsifying obtains pre-emulsion.
(5) under nitrogen protection, pour the pre-emulsion that step (4) is obtained into four-hole boiling flask stirring, be slowly added to cause
Agent sodium sulfite, is warming up to 65 DEG C of reaction 3h, then cools to 45 DEG C, adds rp-emulsification agent, reacts half an hour, then discharges
It is drying to obtain the acrylic thickener of electrolyte-resistant.
Embodiment 2
A kind of paint thickener for printing of electrolyte-resistant, by weight, including following components：
25 parts of acrylic monomerss；
44.3 parts of PH regulators；
20 parts of oil phase solvent；
0.038 part of cross-linking agent；
0.01 part of initiator；
2.0 parts of emulsifying agent；
2.0 parts of rp-emulsification agent；
0.42 part of comonomer；
Its preparation method is comprised the following steps：
(1) under conditions of stirring, PH regulators are slowly added dropwise, acrylic monomerss is neutralized to, persistently stirring makes neutralization
Temperature is less than 40 DEG C.
(2) initiator ammonium persulfate and cross-linking agent are added in the solution neutralized to step (1), water phase is obtained.
(3) oil phase solvent, emulsifying agent and comonomer are mixed, high-speed stirred obtains oil phase.
(4) the oil phase mixing that the water phase and step (3) for obtaining step (2) is obtained, high speed emulsifying obtains pre-emulsion.
(5) under nitrogen protection, pour the pre-emulsion that step (4) is obtained into four-hole boiling flask stirring, be slowly added to cause
Agent sodium sulfite, is warming up to 65 DEG C of reaction 3h, then cools to 45 DEG C, adds rp-emulsification agent, reacts half an hour, then discharges
It is drying to obtain the acrylic thickener of electrolyte-resistant.
Embodiment 3
A kind of paint thickener for printing of electrolyte-resistant, by weight, including following components：
30 parts of acrylic monomerss；
53.3 parts of PH regulators；
24 parts of oil phase solvent；
0.045 part of cross-linking agent；
0.12 part of initiator；
2.4 parts of emulsifying agent；
2.4 parts of rp-emulsification agent；
0.48 part of comonomer；
Its preparation method is comprised the following steps：
(1) under conditions of stirring, PH regulators are slowly added dropwise, acrylic monomerss is neutralized to, persistently stirring makes neutralization
Temperature is less than 40 DEG C.
(2) initiator ammonium persulfate and cross-linking agent are added in the solution neutralized to step (1), water phase is obtained.
(3) oil phase solvent, emulsifying agent and comonomer are mixed, high-speed stirred obtains oil phase.
(4) the oil phase mixing that the water phase and step (3) for obtaining step (2) is obtained, high speed emulsifying obtains pre-emulsion.
(5) under nitrogen protection, pour the pre-emulsion that step (4) is obtained into four-hole boiling flask stirring, be slowly added to cause
Agent sodium sulfite, is warming up to 65 DEG C of reaction 3h, then cools to 45 DEG C, adds rp-emulsification agent, reacts half an hour, then discharges
It is drying to obtain the acrylic thickener of electrolyte-resistant.
Embodiment 4
A kind of paint thickener for printing of electrolyte-resistant, in parts by weight, including following components：
30 parts of acrylic monomerss；
53.3 parts of PH regulators；
24 parts of oil phase solvent；
0.042 part of cross-linking agent；
0.12 part of initiator；
2.4 parts of emulsifying agent；
2.4 parts of rp-emulsification agent；
0.35 part of comonomer；
Its preparation method is comprised the following steps：
(1) under conditions of stirring, PH regulators are slowly added dropwise, acrylic monomerss is neutralized to, persistently stirring makes neutralization
Temperature is less than 40 DEG C.
(2) initiator ammonium persulfate and cross-linking agent are added in the solution neutralized to step (1), water phase is obtained.
(3) oil phase solvent, emulsifying agent and comonomer are mixed, high-speed stirred obtains oil phase.
(4) the oil phase mixing that the water phase and step (3) for obtaining step (2) is obtained, high speed emulsifying obtains pre-emulsion.
(5) under nitrogen protection, pour the pre-emulsion that step (4) is obtained into four-hole boiling flask stirring, be slowly added to cause
Agent sodium sulfite, is warming up to 65 DEG C of reaction 3h, then cools to 45 DEG C, adds rp-emulsification agent, reacts half an hour, then discharges
It is drying to obtain the acrylic thickener of electrolyte-resistant.
Thickening capabilities and electrolyte-resistant ability to the paint thickener for printing of electrolyte-resistant obtained in the present invention are surveyed
Examination, and contrasted with commercially available PTF thickening agents.
Test result is as shown in Table 1 and Table 2：
Table 1
Table 2
From Tables 1 and 2, the paint thickener for printing of the obtained electrolyte-resistant of the present invention under less volume, just
With excellent thickening capabilities and electrolyte resistance, and electrolyte-resistant ability is better than commercially available PTF thickening agents.
Claims (9)
1. a kind of paint thickener for printing of electrolyte-resistant, it is characterised in that：The thickening agent by acrylic monomerss, pH adjusting agent,
Oil phase solvent, cross-linking agent, initiator, emulsifying agent, rp-emulsification agent, comonomer synthesis, by weight, consisting of：
2. electrolyte-resistant paint thickener for printing according to claim 1, it is characterised in that：Described PH regulators are
20-30% sodium hydroxide solutions.
3. electrolyte-resistant paint thickener for printing according to claim 1, it is characterised in that：Described oil phase solvent is nothing
Taste kerosene.
4. electrolyte-resistant paint thickener for printing according to claim 1, it is characterised in that：Described cross-linking agent is N, N-
The double ammoniums of methylene acrylic acid.
5. electrolyte-resistant paint thickener for printing according to claim 1, it is characterised in that：Described initiator is over cure
Sour ammonium, sodium sulfite.
6. electrolyte-resistant paint thickener for printing according to claim 1, it is characterised in that：Described emulsifying agent is
span-80。
7. electrolyte-resistant paint thickener for printing according to claim 1, it is characterised in that：Described rp-emulsification agent is
Tween-80。
8. electrolyte-resistant paint thickener for printing according to claim 1, it is characterised in that：Described comonomer is third
The fat of olefin(e) acid 18.
9. the preparation method of the electrolyte-resistant paint thickener for printing according to any claim in claim 1 to 8, its
It is characterised by, comprises the following steps：
(1) under conditions of stirring, PH regulators are slowly added dropwise, acrylic monomerss is neutralized, persistently stirring makes neutral temperature not
More than 40 DEG C.
(2) initiator ammonium persulfate and cross-linking agent are added in the solution neutralized to step (1), water phase is obtained.
(3) oil phase solvent, emulsifying agent and comonomer are mixed, high-speed stirred obtains oil phase.
(4) the oil phase mixing that the water phase and step (3) for obtaining step (2) is obtained, high speed emulsifying obtains pre-emulsion.
(5) under nitrogen protection, pour the pre-emulsion that step (4) is obtained into four-hole boiling flask stirring, be slowly added to initiator sub-
Sodium bisulfate, is warming up to 65 DEG C of reaction 3h, then cools to 45 DEG C, adds rp-emulsification agent, reacts half an hour, and then discharge drying
Obtain final product the acrylic thickener of electrolyte-resistant.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611107218.2A CN106589207B (en) | 2016-12-06 | 2016-12-06 | A kind of paint thickener for printing of electrolyte-resistant |
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| CN201611107218.2A CN106589207B (en) | 2016-12-06 | 2016-12-06 | A kind of paint thickener for printing of electrolyte-resistant |
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| CN106589207B CN106589207B (en) | 2019-01-15 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107955094A (en) * | 2017-10-31 | 2018-04-24 | 常州菲胜图自动化仪器有限公司 | A kind of preparation method of electrolyte-resistant type hydrophobic association thickener |
| CN111138612A (en) * | 2020-01-10 | 2020-05-12 | 成都德美精英化工有限公司 | Printing thickener and preparation method thereof |
| CN111944086A (en) * | 2020-09-04 | 2020-11-17 | 武汉纺织大学 | Nonionic and alkaline structure modified polyacrylic acid thickening agent and preparation method thereof |
| CN111978458A (en) * | 2020-09-04 | 2020-11-24 | 武汉纺织大学 | Polyacrylic acid thickening agent modified by nonionic side chain and side group and preparation method thereof |
| CN114000367A (en) * | 2021-11-09 | 2022-02-01 | 苏州联胜化学有限公司 | Electrolyte-resistant emulsifying thickener and preparation method thereof |
| CN115198543A (en) * | 2022-07-18 | 2022-10-18 | 苏州联胜化学有限公司 | High-performance pigment printing synthetic thickener and preparation method thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107955094A (en) * | 2017-10-31 | 2018-04-24 | 常州菲胜图自动化仪器有限公司 | A kind of preparation method of electrolyte-resistant type hydrophobic association thickener |
| CN111138612A (en) * | 2020-01-10 | 2020-05-12 | 成都德美精英化工有限公司 | Printing thickener and preparation method thereof |
| CN111944086A (en) * | 2020-09-04 | 2020-11-17 | 武汉纺织大学 | Nonionic and alkaline structure modified polyacrylic acid thickening agent and preparation method thereof |
| CN111978458A (en) * | 2020-09-04 | 2020-11-24 | 武汉纺织大学 | Polyacrylic acid thickening agent modified by nonionic side chain and side group and preparation method thereof |
| CN111944086B (en) * | 2020-09-04 | 2021-12-24 | 武汉纺织大学 | Polyacrylic acid thickener and preparation method thereof |
| CN114000367A (en) * | 2021-11-09 | 2022-02-01 | 苏州联胜化学有限公司 | Electrolyte-resistant emulsifying thickener and preparation method thereof |
| CN114000367B (en) * | 2021-11-09 | 2023-08-04 | 苏州联胜化学有限公司 | Electrolyte-resistant emulsifying thickener and preparation method thereof |
| CN115198543A (en) * | 2022-07-18 | 2022-10-18 | 苏州联胜化学有限公司 | High-performance pigment printing synthetic thickener and preparation method thereof |
| CN115198543B (en) * | 2022-07-18 | 2023-09-12 | 苏州联胜化学有限公司 | High-performance pigment printing synthetic thickener and preparation method thereof |
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| CN106589207B (en) | 2019-01-15 |
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